WO2008019411A1 - Process for the production of a cellulosic fiber from a solution of cellulose in a tertiary amine-oxide and device for carrying out said process - Google Patents
Process for the production of a cellulosic fiber from a solution of cellulose in a tertiary amine-oxide and device for carrying out said process Download PDFInfo
- Publication number
- WO2008019411A1 WO2008019411A1 PCT/AT2007/000377 AT2007000377W WO2008019411A1 WO 2008019411 A1 WO2008019411 A1 WO 2008019411A1 AT 2007000377 W AT2007000377 W AT 2007000377W WO 2008019411 A1 WO2008019411 A1 WO 2008019411A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- filaments
- precipitation bath
- container
- rolls
- process according
- Prior art date
Links
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
Definitions
- the current invention relates to a process for the production of a cellulosic fiber from a solution of cellulose in a tertiary amine-oxide according to claim 1 and a device to carry out such a process according to claim 12.
- Lyocell fibers In recent years, processes have been established which produce cellulose fibers in a mixture of an organic solvent and water. Cellulosic fibers produced from such a solution are called Lyocell fibers. The only profitable process to obtain Lyocell fibers up to now is the production from a tertiary amine oxide solvent, especially from N-methylmorpholine-N-oxide (NMMO). The process yields fibers which are characterized by high strength, a high wet module and improved loop strength, and is commonly known as "amine-oxide process”.
- NMMO N-methylmorpholine-N-oxide
- the shaped article may be prepared by dissolving cellulose in the tertiary amine N-oxide solvent in the barrel of an extrusion apparatus, extruding the solution, orienting by stretching the resulting product in air while still a solution and then precipitating the cellulose from the shaped article before significant degradation of the cellulose.
- the cellulose and tertiary amine N-oxide may be ground to substantially the same particle size before charging the extruder barrel.
- the tertiary amine N-oxide is recovered and recycled to avoid environmental pollution problems.
- the resulting cellulose fibers or films can be used to make fabrics, wrappings or packaging materials or nonwoven products.
- Lyocell fibers nowadays are produced using basically two different techniques.
- a spinning funnel is used which has an outlet in the bottom from which the filaments are drawn off by a drawing force.
- EP 0 574 870 discloses embodiments of this technique. Side streams threatening the fibers to stick together can be avoided by guide plates.
- a second method implies the drawing force to the fibers by mechanical means out of a precipitation bath.
- the drawing-off device is arranged outside the precipitation bath container, such as e.g. shown in US 4,246,221 or WO 93/19230.
- a method and a device for extruding continuous molded bodies is known from WO 02/12599 Al .
- An extrusion solution especially an extrusion solution containing water, cellulose and a tertiary amine oxide, is extruded through an extrusion opening in order to obtain a continuous moulded body and then deviated by means of a deviating device.
- the extrusion openings are arranged in a row in such a way that the individual continuous moulded bodies exit the extrusion head in the form of a curtain in order to enhance the quality of the product. This curtain is then deviated by the deviating device.
- the devices and processes known from the state of the art are restricted concerning the width of the air gap between the spinneret and the precipitation bath, the depth of the precipitation bath and the drawing-off angle of the extruded filaments.
- the latter is an essential factor to the yield and the quality of the fibers. It is defined by the angle between the fibers leaving the spinneret and a horizontal axis. The more openings in the spinneret, the larger the angle will become, the filaments thus tending to stick together or being torn off. On the other hand, a smaller number of openings reduces the yield of the device, thus increasing the production cost of the fibers.
- the process for the production of a cellulosic fiber from a solution of cellulose in a tertiary amine-oxide via a jet-wet process comprises the steps of pressing the solution of cellulose through a spinneret, thereby obtaining filaments, conducting the filaments through an air gap into a container containing a precipitation bath, drawing the filaments in the air gap, transporting the filaments out of the precipitation bath, further processing of the filaments, wherein drawing of the filaments is performed via a mechanically driven drawing-off device exerting a drawing force and at least part of the drawing force is transmitted onto the filaments by contacting the filaments with the drawing-off device at a location within the precipitation bath.
- Further processing steps include all steps performed on the filaments including the transport of the filaments after passing the precipitation bath.
- Major steps of processing are cutting and washing of the filaments.
- the device for carrying out a process comprises a spinneret for extruding the solution of cellulose to form cellulose filaments, a container for a precipitation bath located beneath the spinneret and located at a distance from the spinneret such that when the container is filled with the precipitation bath, an air gap between the surface of the precipitation liquid and the surface of the spinneret is formed, a mechanically driven drawing-off device for drawing the filaments in the air gap by means of a drawing force exerted by said drawing-off device wherein the drawing-off device having a contact point at which the filaments are contacted with the device and at which at least part of the drawing force is transmitted onto the filaments.
- the contact point is located within the container for the precipitation bath.
- inventive device and process are characterized by a mechanical drawing-off device which is arranged in the precipitation bath and applies the drawing force to the fiber there.
- Prior art documents show a drawing-off device arranged outside the bath thereby restricting the flexibility for the geometric design of the apparatus. The fiber leaves the bath smooth and drawn to its final length and is immediately ready for further processing without further drawing.
- the entire drawing force is transmitted onto the filaments at said location within the precipitation bath. Since the whole device exerting the drawing force on the filaments is located in the precipitation bath, it is advantageous to restrict drawing to the same area.
- the tensile load in longitudinal direction the filaments are exposed to is less than 5,5 cN/tex.
- the filaments thereby produced have less tendency of fibrillation.
- said drawing-off device is a device selected from the group consisting of rolls, belts, and systems comprising both rolls and belts.
- the rolls and belts are equipped with a filament-contacting surface designed to allow the transmission of at least part of the drawing force by way of adhesion between the filaments and the surface.
- the design of the surface is selected from the group consisting of micro-structured, corrugated, permeable, ribbed and/or expandable design.
- Yet another preferred embodiment of the invention shows the removal of the filaments from the drawing-off device by means of a step selected from the group consisting of flushing with water, shaking, chafing, brushing, sucking and blowing.
- the filaments are deflected in the precipitation bath and transported out of the precipitation bath at a side wall of the precipitation bath container or via the surface of the precipitation bath.
- the filaments are transported out of the precipitation bath in a downward direction at the bottom of the precipitation bath container.
- the drawing-off device is designed such as to essentially prevent leakage of the precipitation bath out of the precipitation bath container.
- the filaments are drawn and transported out of the precipitation bath in the form of a curtain whereby the drawing-off angle is reduced considerably.
- the drawing-off device is a device selected from the group consisting of rolls, belts, and systems comprising both rolls and belts.
- the filament-contacting surface of the rolls or belts, respectively is designed such as to allow the transmission of at least part of the drawing force by way of adhesion between the filaments and the surface, said surface being of a design selected from the group consisting of micro-structured, corrugated, permeable, ribbed and/or expandable design.
- the drawing-off device comprises means for removing the filaments from the drawing-off device, a deflecting means for deflecting the filaments in the precipitation bath, means for transporting the filaments out of the precipitation bath via the surface of the precipitation bath.
- the drawing-off device is located at the bottom of the precipitation bath container and comprises means for transporting the filaments out of the precipitation bath in a downward direction, comprising two rolls located at the bottom of the precipitation bath container or at a side wall of the precipitation bath container, said rolls defining a gap through which the filaments pass when being drawn-off, said gap being defined such as to essentially prevent leakage of the precipitation bath from the container.
- the rolls at the bottom of the container of precipitation bath are arranged to be movable against each other in order to adjust the size of the gap between the rolls.
- the present invention provides a very high degree of flexibility in adapting the geometrical design of the precipitation bath, especially its depth. It is possible to have very low precipitation bath depths. Therefore, in one further aspect of the invention said precipitation bath has a depth, the minimum depth of the container being defined as approximately equal to the radius of the rolls.
- the spinneret preferably is a rectangular spinneret for spinning the filaments in the form of a curtain, wherein the drawing-off device is designed such as to draw and transport the filaments out of the precipitation bath container in the form of a curtain.
- Fig. IA is a schematic side view of a preferred embodiment of the device according to the present invention.
- Fig. IB is a schematic side view of a second embodiment of the device according to the present invention.
- Fig. 2 is a schematic view of a curtain of filaments
- Fig. 3A-B are schematic views of a third and a fourth embodiment of the device according to the present invention.
- Fig. 3C is a schematic view of a fifth embodiment of the device according to the present invention.
- Fig. 4 is a schematic view of a sixth embodiment of the device according to the present invention.
- the process for the production of a cellulosic fiber from a solution of cellulose in a tertiary amine-oxide via a jet- wet process generally comprises several steps which have significant impact on the structure and texture of the filaments.
- a first embodiment of a device 1 suitable for the carrying out of said process is shown in Fig. IA.
- the solution of cellulose is pressed through a spinneret (not shown), which can include one or more openings arranged in different configurations like one or more circles etc.
- the spinneret is a rectangular spinneret for spinning the filaments in the form of a curtain.
- the filaments 2 obtained thereby are conducted through an air gap 3 between the spinneret and a container 4 containing a precipitation bath. While passing the air gap 3, the filaments 2 are drawn to impart improved physical properties like advanced wet moduli thereto.
- the drawing-off angle of the filaments 2 leaving the spinneret is limited for example by the width of the air gap 3. Since the drawing-off angle defined by the angle between the filaments 2 leaving the spinneret and a horizontal axis is an essential factor for the yield and the quality of the fibers it is desireable to keep it as small as possible. The more openings in the spinneret, the larger the angle will become, the filaments thus tending to stick together or being torn off when the air gap 3 is too narrow. On the other hand, a smaller number of openings reduces the yield of the device, thus increasing the production costs of the fibers.
- the invention thus allows to use spinnerets with more outlet openings since the air gap 3 or the depth of the precipitation bath can be wider or deeper respectively compared to the devices of the prior art.
- the drawing of the filaments 2 is performed via a mechanically driven drawing-off device 5 exerting a drawing force on the filaments 2.
- the device 5 exerting the drawing force is driven mechanically, in contrast to funnel -spinning where the drawing force is exerted by the co-current stream of precipitation liquid. Afterwards the filaments 2 are transported out of the precipitation bath container 4 and further processed.
- At least part of the drawing force is transmitted onto the filaments 2 by contacting the filaments 2 with the drawing-off device 5 at a location within the container 4 containing the precipitation bath. More specific, a contact point C of the filaments 2 with the drawing-off device 5 is located within the precipitation bath or rather under the surface of the precipitation bath solution. Preferably the entire drawing force can be exerted onto the filaments 2 at said contact point C within the precipitation bath.
- the tensile load in longitudinal direction the filaments 2 are exposed to is in preferably less than 5,5 cN/tex during further processing, i.e. after having been drawn. Thus the filaments have less tendency for fibrillation during further processing.
- Further processing steps include all steps performed on the filaments 2 including the transport of the filaments 2 after passing the first contact point C.
- Major steps of processing are cutting and washing of the filaments 2.
- the drawing-off device 5 is a device selected from the group consisting of rolls 6 and belts 7 as well as systems comprising both rolls 6 and belts 7.
- the embodiment according Fig. IA comprises two rolls 6 and a belt 7 connecting the rolls 6, while a second embodiment according to Fig. IB comprises seven rolls 6 arranged in two groups by two belts 7.
- the stretching force exerted on the filaments 2 can be controlled.
- This is especially enabled by movably mounted rolls 6 as indicated in Fig. I B.
- the contact point C is located on a roll 6 located near the bottom of the precipitation bath container 4, but alternatively the contact point C can be located at the topmost pair of rolls 6". This enables an exertion of the drawing force in the upper part of the precipitation bath container 4 and a subsequent passage of the filaments 2 through the precipitation bath without further stretching.
- the drawing-off device 5 is designed such as to draw and transport the filaments 2 out of the precipitation bath container 4 in the form of a curtain. It is also possible to use a plurality of rectangular spinnerets producing a plurality of parallel curtains of filaments 2. The curtains are guided through the precipitation bath similar to a single curtain of filaments 2.
- Rolls 6 and/or belts 7 are equipped with a surface 8 contacting the filaments 2.
- the surface 8 of the rolls 6 and/or belts 7 is designed to allow the transmission of a part of the drawing force or the entire drawing-force by way of adhesion between the filaments 2 and the surface 8, the design of the surface 8 being micro-structured, corrugated, permeable, ribbed and/or expandable.
- Fig. 2 shows a very schematic view from above on a group of filaments 2 deviated by a roll 6 and transported by a belt 7. The filaments 2 stick to the belt 7 until they are removed.
- a ribbed surface can be designed in different ways; on the one hand, tops of the ribbed structure of one roll surface can meet corresponding depressions of the opposite roll surface, on the other hand, the tops of the corresponding surface structures can come in contact during rotation of the rolls 6.
- Said means for removal are necessary.
- Said means can for example flush the filaments 2 off the surface 8 by water, the beam of water assuming various shapes.
- Other possibilities can be of mechanical nature like shaking, reloading, sucking or blowing or removal by auxiliary means like chafers or brushes.
- FIG. 3 A through 3C Further embodiments of devices 1 for the processing of the filaments 2 in the container 4 of the precipitation bath transporting the filaments 2 out of the precipitation bath in a downward direction at the bottom of the precipitation bath container 4 are shown in Figs. 3 A through 3C, where the drawing-off device 5 is arranged at the bottom of the container 4 and is designed such as to essentially prevent leakage of the precipitation bath out of the precipitation bath container 4.
- the drawing-off device 5 When the drawing-off device 5 is located at the bottom of the precipitation bath container 4, it comprises means for transporting the filaments out of the precipitation bath in a downward direction.
- Those means are represented by two rolls 12 located at the bottom of the precipitation bath container 4 or at a side wall of the precipitation bath container 4, said rolls 12 defining a gap 11 between them through which the filaments 2 pass when being drawn-off.
- Said gap 1 1 is adequately dimensioned to essentially prevent leakage of the precipitation bath from the container 4.
- said rolls 12 are arranged movably against each other in order to adjust the size of the gap 1 1 between the rolls 12 according to the thickness of the filaments 2 or curtain of filaments 2.
- Figs. 3 A through 3C illustrate various possibilities of design regarding the number of rolls 6 and belts 7 ranging from the simple embodiment according to Fig. 3 A containing only the two rolls 12, over an embodiment according to Fig. 3B containing two rolls 6 for deflection connected to the two rolls 12 by two belts 7, to an arrangement according to Fig. 3C showing an elongated design to allow further processing of the filaments 2 leaving the container 4, for example by applying a treatment fluid.
- the filaments 2 deflected in the precipitation bath by means of deflection 10 can be transported out of the precipitation bath container 4 through a side wall 9 of the precipitation bath container 4 according to Fig. 4 or via the surface of the precipitation bath.
- the latter alternative is shown in Figs. IA and IB, the means of deflection 10 there being represented by the rolls 6, especially by a bottommost roll 6'.
- Said bottommost roll 6' is preferably the roll by which the contact point C of the filaments 2 with the drawing-off device 5 is marked.
- the minimum depth of the precipitation bath container 4 of all embodiments described above is only limited by a radius R of the rolls 6.
- the minimum depth of the container 4 is approximately equal to the radius R of the rolls 6 at which the contact point C is located.
- a typical value for the radius R and the respective minimum depth of the container 4 may be approximately 6 cm.
- the device 1 can be significantly reduced in size by this, requiring less space.
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE112007001828T DE112007001828T5 (en) | 2006-08-17 | 2007-08-06 | A process for producing a cellulose fiber from a solution of cellulose in a tertiary amine oxide and apparatus for carrying out the process |
CN2007800306157A CN101506410B (en) | 2006-08-17 | 2007-08-06 | Process for the production of a cellulosic fiber from a solution of cellulose in a tertiary amine-oxide and device for carrying out said process |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
ATA1381/2006 | 2006-08-17 | ||
AT13812006A AT504144B1 (en) | 2006-08-17 | 2006-08-17 | METHOD FOR THE PRODUCTION OF CELLULOSE FIBERS FROM A SOLUTION OF CELLULOSE IN A TERTIARY AMINE OXIDE AND DEVICE FOR CARRYING OUT THE METHOD |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2008019411A1 true WO2008019411A1 (en) | 2008-02-21 |
Family
ID=38662832
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/AT2007/000377 WO2008019411A1 (en) | 2006-08-17 | 2007-08-06 | Process for the production of a cellulosic fiber from a solution of cellulose in a tertiary amine-oxide and device for carrying out said process |
Country Status (4)
Country | Link |
---|---|
CN (1) | CN101506410B (en) |
AT (1) | AT504144B1 (en) |
DE (1) | DE112007001828T5 (en) |
WO (1) | WO2008019411A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3505659A1 (en) | 2018-08-30 | 2019-07-03 | Aurotec GmbH | Method and device for filament spinning with inflection |
CN116334777A (en) * | 2023-05-26 | 2023-06-27 | 吉林富博纤维研究院有限公司 | Water bath drafting device and PAN-based carbon fiber precursor production system |
Citations (6)
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GB1051472A (en) * | 1963-02-26 | |||
GB929655A (en) * | 1959-11-02 | 1963-06-26 | Tachikawa Res Inst | Process for producing viscose rayon filamentary material |
US5234651A (en) * | 1991-09-12 | 1993-08-10 | Kigen Kawai | Dry-jet wet spinning of fibers including two steps of stretching before complete coagulation |
WO1993019230A1 (en) * | 1992-03-17 | 1993-09-30 | Lenzing Aktiengesellschaft | Process for manufacturing cellulose moulded bodies and a device for carrying it out |
WO1997023667A1 (en) * | 1995-12-21 | 1997-07-03 | Courtaulds Fibres (Holdings) Limited | Fibre manufacture |
WO2004088010A1 (en) * | 2003-04-01 | 2004-10-14 | Zimmer Aktiengesellschaft | Method and device for producing post-stretched cellulose spun threads |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
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US3996321A (en) * | 1974-11-26 | 1976-12-07 | E. I. Du Pont De Nemours And Company | Level control of dry-jet wet spinning process |
US4416698A (en) * | 1977-07-26 | 1983-11-22 | Akzona Incorporated | Shaped cellulose article prepared from a solution containing cellulose dissolved in a tertiary amine N-oxide solvent and a process for making the article |
US4246221A (en) | 1979-03-02 | 1981-01-20 | Akzona Incorporated | Process for shaped cellulose article prepared from a solution containing cellulose dissolved in a tertiary amine N-oxide solvent |
DE4308524C1 (en) | 1992-06-16 | 1994-09-22 | Thueringisches Inst Textil | Process for the production of cellulose fibers and filaments by the dry-wet extrusion process |
ATA239194A (en) * | 1994-12-22 | 1996-02-15 | Chemiefaser Lenzing Ag | DEVICE FOR CARRYING OUT A DRY / WET SPINNING PROCESS |
AT404032B (en) | 1996-03-04 | 1998-07-27 | Chemiefaser Lenzing Ag | METHOD FOR PRODUCING CELLULOSIC FIBERS |
AT406386B (en) * | 1998-07-28 | 2000-04-25 | Chemiefaser Lenzing Ag | METHOD AND DEVICE FOR PRODUCING CELLULOSIC MOLDED BODIES |
DE10037923A1 (en) | 2000-08-03 | 2001-03-29 | Zimmer Ag | Extrusion of solutions based on water cellulose and tertiary amine oxide to create continuous fibers, involves forming a flat band of fibers which passes around a diverter |
DE102004031025B3 (en) * | 2004-06-26 | 2005-12-29 | Thüringisches Institut für Textil- und Kunststoff-Forschung e.V. | Method and device for the production of shaped articles from cellulose |
DE102005024433A1 (en) * | 2005-05-24 | 2006-02-16 | Zimmer Ag | Lyocell staple fibers of increased loop strength are obtained by having tertiary amine oxides still present in the spun filaments during the cutting stage |
-
2006
- 2006-08-17 AT AT13812006A patent/AT504144B1/en not_active IP Right Cessation
-
2007
- 2007-08-06 DE DE112007001828T patent/DE112007001828T5/en not_active Withdrawn
- 2007-08-06 WO PCT/AT2007/000377 patent/WO2008019411A1/en active Application Filing
- 2007-08-06 CN CN2007800306157A patent/CN101506410B/en not_active Expired - Fee Related
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB929655A (en) * | 1959-11-02 | 1963-06-26 | Tachikawa Res Inst | Process for producing viscose rayon filamentary material |
GB1051472A (en) * | 1963-02-26 | |||
US5234651A (en) * | 1991-09-12 | 1993-08-10 | Kigen Kawai | Dry-jet wet spinning of fibers including two steps of stretching before complete coagulation |
WO1993019230A1 (en) * | 1992-03-17 | 1993-09-30 | Lenzing Aktiengesellschaft | Process for manufacturing cellulose moulded bodies and a device for carrying it out |
WO1997023667A1 (en) * | 1995-12-21 | 1997-07-03 | Courtaulds Fibres (Holdings) Limited | Fibre manufacture |
WO2004088010A1 (en) * | 2003-04-01 | 2004-10-14 | Zimmer Aktiengesellschaft | Method and device for producing post-stretched cellulose spun threads |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3505659A1 (en) | 2018-08-30 | 2019-07-03 | Aurotec GmbH | Method and device for filament spinning with inflection |
WO2020043860A1 (en) | 2018-08-30 | 2020-03-05 | Aurotec Gmbh | Method and device for filament spinning with deflection |
US11946165B2 (en) | 2018-08-30 | 2024-04-02 | Aurotec Gmbh | Method and device for filament spinning with deflection |
CN116334777A (en) * | 2023-05-26 | 2023-06-27 | 吉林富博纤维研究院有限公司 | Water bath drafting device and PAN-based carbon fiber precursor production system |
CN116334777B (en) * | 2023-05-26 | 2023-07-21 | 吉林富博纤维研究院有限公司 | Water bath drafting device and PAN-based carbon fiber precursor production system |
Also Published As
Publication number | Publication date |
---|---|
CN101506410A (en) | 2009-08-12 |
CN101506410B (en) | 2011-05-18 |
DE112007001828T5 (en) | 2009-06-25 |
AT504144B1 (en) | 2013-04-15 |
AT504144A1 (en) | 2008-03-15 |
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